Correlations between a materials microstructure and mechanical behavior are important for materials development. As materials characterization methods must consider instrument accessibility, sample dimensions and economical aspects, developing functional techniques in order to obtain better understanding of materials behavior in micro and nano scale is crucial. Procedures for assessing and interpreting the mechanical responses at small scales, combined with investigating the microstructure, are considered as significant steps to design and develop the effective frameworks for evaluating bulk properties. This research demonstrates how fundamental understanding of microstructures can assist interpreting of mechanical performance of bulk materials. Testing of materials at small scales is very important because the mechanical failure of any bulk material starts with the formation, extension, or local accumulation of initially small defects, leading finally to a catastrophic fracture by an expanding crack. Thus, any bulk material profits from an in-depth understanding of its deformation and mechanical phenomena at the nano- and micrometer length scale.<div><br></div><div>This thesis shows how the micro constituents’ interactions and grain boundaries reactions to dislocations in alloys and thin films contribute to understanding material flow behavior and differences in the mechanical properties of these materials in a wide range of material systems with variations in appropriate sizes which need to be probed. Among other things, this work shows that sources of variation can be specified and quantified as predictive tools for designing materials. Several examples are presented. First, the strength and strain hardening of martensite and ferrite in a dual phase steel with a grain size less than 5 μm were determined using an inverse technique. The yield strength of the ferrite and martensite phases are obtained as 370 MPa and 950 MPa respectively. The calculated hardening exponent of the alloy was exactly the same as experimental tensile test results (0.11). The constraint phenomena was effective in restricting deformation of this elastic-plastic alloy. Secondly, the differences in hardness and pop-in behavior were used to understand of the influences of different types of grain boundaries, high density dislocations, and twins in Al thin films before and after plasticity. The third example assesses the strength of several species of diatom frustules for the first time using a combination of indentation techniques. Lightweight materials with densities well below 1000 kg/m3 demonstrated strengths on the order of 100’s of MPa. Finally, conditions for laser grown oxides and laser shock peening on a commercial steel which lead to an optical marking without a change in strength around the marking have been identified.<br></div>

Zirconium alloys (zircaloy) have been widely used in light water reactors due to their good thermomechanical properties, corrosion resistance, and low thermal neutron absorption rate. As one of the most important safety barriers, cladding is not only used to encapsulate nuclear fuel, but also to prevent the nuclear fission products from leaking into the coolant. During the operation of nuclear reactors, hydride will form in zircaloy and significantly degrade the tensile strength, ductility, fracture toughness, and creep behavior of the cladding, and eventually leading to the failure of cladding. Therefore, understanding the material properties of zircaloy and its hydrides is crucial to the safety of power plants. In this study, the mechanical Raman spectroscopy and nano-mechancial testing techniques were used to perform thermomechanical measurements and damage analysis of zircaloy-4. The Raman thermometry method was used to measure localized spatially resolved thermal conductivity and establish the potential linkage of microstructure to thermal and mechanical properties of zircaloy-4. The local thermal conductivity values showed to increase with increase in grain size. Nanoindentation and nano-scale impact techniques were used to obtain the viscoplastic constitutive relation of hydrides at elevated temperatures. Based on the obtained viscoplastic model, fracture strength of hydrides was predicted by using finite element method (FEM) simulations. An extended Gurson-Tvergaard-Needleman (GTN) model was used to study the macro-scale fracture behavior of hydrided zircaloy-4 structures. Good agreement between calculated and experimental results was obtained for various boundary conditions.

Mechanical surface treatments using an elastic-plastic cold working process can develop residual stresses on the surface of a workpiece. Compressive residual stresses on the surface increase resistance against surface crack propagation, so the overall mechanical performance can be improved by this technique. Compressive residual stresses can be created by different methods such as hammering, rolling, and shot peening. Shot peening is a well-established method to induce compressive residual stresses in the metallic components using cold working, and often ascribed to being beneficial to fatigue life in the aerospace and automobile industries. In this method, the surface is bombarded by high-velocity spherical balls which cause plastic deformation of the substrate, leading to a residual compressive stress after shot peening on the surface of the part. Computational modeling is an appropriate and effective way which can predict the amount of produced residual stresses and plastic deformation to obtain surface roughness after shot peening simulation. Finally, an experimental method to measure the magnitude of the residual stress using a nanoindentation technique was developed. The experimental indentation method was compared to both computational predictions (in aluminum) and with x-ray diffraction measurements of stress (in an alloy steel). The current study validates the relation between the nanoindentation method and numerical simulation for assessing the surface residual stresses resulting from single or multiple shot peening processes.

<p> This dissertation describes the recent advancements in micromechanical testing that inform how deformation mechanisms in austenitic stainless steels (SS) are affected by the presence of irradiation-induced defects. Austenitic SS is one of the most widely utilized structural alloys in nuclear energy systems, but the role of irradiation on its underlying mechanisms of mechanical deformation remains poorly understood. Now, recent advancement of microscale mechanical testing in a scanning electron microscope (SEM), coupled with site-specific transmission electron microscopy (TEM), enables us to precisely determine deformation mechanisms as a function of plastic strain and grain orientation.</p> <p> </p> <p>We focus on AISI 304L SSs irradiated in EBR-II to ~1-28 displacements per atom (dpa) at ~415 °C and contains ~0.2-8 atomic parts per million (appm) He amounting to ~0.2-2.8% swelling. A portion of the specimen is laser welded in a hot cell; the laser weld heat affected zone (HAZ) is studied and considered to have undergone post-irradiation annealing (PIA). An archival, virgin specimen is also studied as a control. We conduct nanoindentation, then prepare TEM lamellae from the indent plastic zone. In the 3 appm He condition, TEM investigation reveals nucleation of deformation-induced <i>α</i>’ martensite in the irradiated specimen, and metastable <i>ε</i> martensite in the PIA specimen. Meanwhile, the unirradiated control specimen exhibits evidence only of dislocation slip and twinning; this is unsurprising given that alternative deformation mechanisms such as twinning and martensitic transformation are typically observed only near cryogenic temperatures in austenitic SS. Surface area of irradiation-produced cavities contribute enough free energy to accommodate the martensitic transformation. The lower population of cavities in the PIA material enables metastable <i>ε</i> martensite formation, while the higher cavity number density in the irradiated material causes direct <i>α</i>’ martensite formation. In the 0.2 appm He condition, SEM-based micropillar compression tests confirm nanoindentation results. A deformation transition map with corresponding criteria has been proposed for tailoring the plasticity of irradiated steels. Irradiation damage could enable fundamental, mechanistic studies of deformation mechanisms that are typically only accessible at extremely low temperatures. </p>